CN102062710B - Preparation method of observation sample for transmission electron microscope - Google Patents
Preparation method of observation sample for transmission electron microscope Download PDFInfo
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- CN102062710B CN102062710B CN200910198939A CN200910198939A CN102062710B CN 102062710 B CN102062710 B CN 102062710B CN 200910198939 A CN200910198939 A CN 200910198939A CN 200910198939 A CN200910198939 A CN 200910198939A CN 102062710 B CN102062710 B CN 102062710B
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Abstract
The invention provides a preparation method of an observation sample for a transmission electron microscope, which comprises the following steps: the preparation of a testing structure, comprising: firstly, forming two rows of mark holes mutually in parallel in the course of manufacturing wafers, wherein the distance between the opposite edges of the two rows of the mark holes is the thickness of the observation sample finally obtained, and the graphic region to be observed is in parallel to the two rows of the mark holes and is arranged in the region between the two roles of the mark holes; and secondly, the deposition of the metal with obvious secondary electron image contrast and the preparation of the observation sample, comprising: eliminating the surface in parallel to the graphic region to be observed on the testing structure layer by layer and stopping the elimination action until after completely eliminating the tow rows of the mark holes, thereby obtaining the final observation sample. The preparation method of the observation sample for the transmission electron microscope can accurately judge the cutting stopping point through the mark holes and cannot cause the excessive cutting.
Description
Technical field
The present invention relates to semiconductor fabrication and material analysis field, particularly a kind of transmission electron microscopy observation sample preparation methods.
Background technology
Transmission electron microscope (transmission electron microscope; TEM) be IC industry observation very important instrument of micromechanism and means; It as light source, makes lens with electromagnetic field with high-power electron beam, will pass through the electron beam that quickens and assemble and project on the extremely thin sample; Atom in electronics and the sample changes direction because of collision, thereby produces the solid angle scattering.The size of scattering angle and the density of sample, thickness are relevant, therefore can form the different image of light and shade.Since the penetration power of electron beam very a little less than, the sample that therefore is used for Electronic Speculum must be processed the ultra-thin section about the about 100nm of thickness.
In the prior art, when preparation is used for the observing samples of transmission electron microscope, adopts mechanical lapping usually or focus on example bundle (FIB) sample is cut attenuate.The method of use mechanical lapping can not cause damage to observing samples when preparing observing samples, but this method can't realize accurate location; Can accurately locate the position and the mode of cutting sample when using FIB to prepare sample, but the observing samples thickness for preparing in the prior art can only accomplish generally about 100nm, be difficult to prepare thinner observing samples.
Please referring to Fig. 1, the transmission electron microscopy observation sample synoptic diagram that Fig. 1 prepares when being wider than 100nm for graph line.As shown in Figure 1, like the sectional view looks of need observation active area 1, if the live width of active area 1 is 200nm, during the transmission electron microscopy observation sample of preparation active area 1, available FIB cuts active area 1, makes its thickness reduce to 100nm.Therefore, simpler during the observing samples of preparation transmission electron microscope under the bigger situation of figure live width, be easy to grasp.
But along with the exploitation of semicon industry advanced process, the critical size of device is more and more littler.When processing procedure is 90nm or 90nm when following, the live width of figure maybe be much smaller than the transmission electron microscopy observation sample thickness.This moment, the need observation figure of narrow linewidth structure was not completely contained in the sample probably, also may comprise the unnecessary graphical information of multilayer in the thickness of sample if continue the observing samples that the method for use prior art prepares transmission electron microscope.Please referring to Fig. 2, Fig. 2 is the narrow linewidth figure transmission electron microscopy observation sample synoptic diagram of prior art for preparing.As shown in Figure 2, be similarly the sectional view looks that need observation active area 2, the live width of active area 2 is 50nm.When using the transmission electron microscopy observation sample of this active area 2 of FIB preparation; At first use FIB to carry out first cutting; Need the limit to cut edge during cutting and see, use the ion beam cutting of certain energy to include the cross section of source region 2 figures on one side, Yi Bian with the secondary electron image of electron beam observation cross section structure; When active area 2 structures occur, stop cutting immediately; Next carry out the cutting of second limit again, be thinned to thickness of sample about 100nm.Since in the integrated circuit secondary electron image contrast of the silicon dioxide of the monocrystalline silicon of polysilicon, active area and shallow trench isolation region a little less than; The electron beam patterning of these structures is not easy to distinguish identification; When therefore using FIB cutting preparation observing samples, the terminating point of accurate assurance cutting is difficulty very.When we observed the appearance of active area 2 structures, active area 2 has been cut off a part probably even the overwhelming majority is cut off.Simultaneously; Because active area 2 is much smaller than the TEM thickness of sample; Make in the thickness of observing samples to have comprised multilayer material and structure, just can occur the ghost image phenomenon of unlike material and structure during the cross section of using the transmission electron microscopy observation sample, influence the judgement of image pattern and the measurement of size.
Summary of the invention
The technical matters that the present invention will solve provides a kind of transmission electron microscopy observation sample preparation methods, can't accurately define the problem of sample cutting halt when preparing sample to solve.
For solving the problems of the technologies described above, a kind of transmission electron microscopy observation sample preparation methods of the present invention may further comprise the steps:
The preparation test structure; Comprise: at first; In wafer production process, form the index aperture that two rows are parallel to each other, said two row's index aperture distance between the edge in opposite directions are the thickness of the observing samples that finally need obtain; Need the observation graphics field to be parallel to said two row's index aperture, and in the zone between said two row's index aperture; Secondly, the tangible metal of deposit secondary electron image contrast in said index aperture;
The preparation observing samples comprises: successively remove on the said test structure and need observe parallel surface, graphics field with said, after removing said two row's index aperture fully, stop to remove action, obtain final observing samples.
Optional, said every row's index aperture comprises one or more index aperture.
Optional, said index aperture be shaped as column, bulk, sphere or linear.
Optional, the method that forms said index aperture is an etching.
Optional, the method for depositing metal comprises chemical vapor deposition, physical vapour deposition (PVD), electrochemical deposition in said index aperture.
Optional, successively remove on the said test structure and be: adopt FIB successively to cut to remove on the said test structure and the said observation parallel surface, graphics field that needs with the said method on parallel surface, observation graphics field that needs.
Transmission electron microscopy observation sample preparation methods of the present invention is outside the cross section of the observing samples that need obtain; Distance about about 100nm forms the index aperture that is filled with metal; Because the secondary electron image contrast of metal is more outstanding in the index aperture, therefore, when preparing observing samples with FIB; Can accurately arrive this index aperture cross section, after cutting away index aperture fully, stop cutting through the secondary beam imaging observation.Transmission electron microscopy observation sample preparation methods of the present invention can clearly be judged the cutting halt through this index aperture, can not cause excessive cutting.This method is particularly useful for preparing the transmission electron microscopy observation sample of narrow linewidth figure; Through the prior mark cutting of index aperture halt; Can effectively prevent because excessive cutting causes the contrast of required observation figure in the observing samples to be covered; Prevent that the ghost image phenomenon of unlike material and aspect from appearring in image, thereby judge pattern and measurement size more accurately.
Description of drawings
The transmission electron microscopy observation sample synoptic diagram that Fig. 1 prepares when being wider than 100nm for graph line;
Fig. 2 is the method synoptic diagram of prior art for preparing narrow linewidth figure transmission electron microscopy observation sample;
Fig. 3 a-Fig. 3 b prepares the method synoptic diagram of transmission electron microscopy observation sample for adopting the inventive method.
Embodiment
For make above-mentioned purpose of the present invention, feature and advantage can be more obviously understandable, does detailed explanation below in conjunction with the accompanying drawing specific embodiments of the invention.
A kind of transmission electron microscopy observation sample preparation methods of the present invention multiple substitute mode capable of using realizes; Be to explain below through preferred embodiment; Certainly the present invention is not limited to this specific embodiment, and the general replacement that the one of ordinary skilled in the art knew is encompassed in protection scope of the present invention undoubtedly.
Secondly, the present invention utilizes synoptic diagram to describe in detail, and when the embodiment of the invention was detailed, for the ease of explanation, synoptic diagram disobeyed that general ratio is local amplifies, should be with this as to qualification of the present invention.
Please referring to Fig. 3 a-Fig. 3 b, Fig. 3 a-Fig. 3 b is for adopting the transmission electron microscopy observation sample synoptic diagram of the inventive method preparation.Shown in Fig. 3 a, transmission electron microscopy observation sample preparation methods of the present invention may further comprise the steps:
At first, preparation test structure 3 comprises: at first; In wafer production process; Form the index aperture 7 that two rows are parallel to each other, said two row's index aperture 7 distance between the edge in opposite directions need the observation graphics field be parallel to said two row's index aperture 7 for the thickness 8 of the observing samples that finally need obtain; And in the zone of said two rows between the index aperture 7 (shown in Fig. 3 a, the cross section 6 that needs the observation graphics field between said two row's index aperture 7 tops in regional 5); Secondly, the tangible metal of deposit secondary electron image contrast in said index aperture 7;
Said need the observation graphics field be the plane perpendicular to paper shown in the dotted line 4 among Fig. 3 a.
In the prior art, be applicable to that the thickness 8 of the observing samples of transmission electron microscope is generally about 100nm.
Said every row's index aperture 7 comprises one or more index aperture.The shape of said index aperture 7 can be column, bulk, sphere or linear etc.The method that forms said index aperture 7 can be lithographic method of the prior art etc.
The method of depositing metal comprises chemical vapor deposition, electrochemical deposition or physical vapour deposition (PVD) etc. in said index aperture 7, but the tangible metals of secondary electron contrast such as deposition tungsten, platinum in the said index aperture 7.
Secondly, the preparation observing samples comprises: successively remove on the said test structure 3 and need observe parallel surface, graphics field with said, after removing said two row's index aperture 7 fully, stop to remove action, obtain final observing samples.
Successively remove on the said test structure 3 and be: adopt FIB successively to cut on the said test structure 3 of removal and need observe parallel surface, graphics field with said with the said method on parallel surface, graphics field of need observing.
So far, shown in Fig. 3 b, said test structure 3 becomes and is applicable to transmission electron microscope, can be to the said observing samples that needs the observation graphics field to observe.
Transmission electron microscopy observation sample preparation methods of the present invention is outside the cross section of the observing samples that need obtain; Distance about about 100nm forms the index aperture that is filled with metal, because the electron beam patterning contrast of metal is more outstanding in the index aperture, therefore; When the preparation observing samples; When being cut to the cross section of index aperture, can accurately observing this index aperture cross section, thereby stop cutting through electron beam patterning.Transmission electron microscopy observation sample preparation methods of the present invention can clearly be judged the cutting halt through this index aperture, can not cause excessive cutting.This method is particularly useful for preparing the transmission electron microscopy observation sample of narrow linewidth figure; Through the prior mark cutting of index aperture halt; Can effectively prevent because excessive grinding or cutting cause comprising in the thickness of observing samples other and unwanted figure; Prevent that the ghost image phenomenon of unlike material and aspect from appearring in image, thereby judge pattern and measurement size more accurately.
Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.Like this, belong within the scope of claim of the present invention and equivalent technologies thereof if of the present invention these are revised with modification, then the present invention also is intended to comprise these changes and modification interior.
Claims (5)
1. transmission electron microscopy observation sample preparation methods may further comprise the steps:
The preparation test structure; Comprise: at first; In wafer production process, form the index aperture that two rows are parallel to each other, said two row's index aperture distance between the edge in opposite directions are the thickness of the observing samples that finally need obtain; Need the observation graphics field to be parallel to said two row's index aperture, and in the zone between said two row's index aperture; Secondly, the tangible metal of deposit secondary electron image contrast in said index aperture;
The preparation observing samples comprises: adopt FIB successively to cut on the said test structure of removal and need observe parallel surface, graphics field with said, after removing said two row's index aperture fully, stop to remove and move, obtain final observing samples.
2. transmission electron microscopy observation sample preparation methods as claimed in claim 1 is characterized in that, every row's index aperture comprises one or more index aperture.
3. according to claim 1 or claim 2 transmission electron microscopy observation sample preparation methods is characterized in that, said index aperture be shaped as column, bulk, sphere or linear.
4. transmission electron microscopy observation sample preparation methods as claimed in claim 1 is characterized in that, the method that forms said index aperture is an etching.
5. transmission electron microscopy observation sample preparation methods as claimed in claim 1 is characterized in that the method for depositing metal comprises chemical vapor deposition, physical vapour deposition (PVD), electrochemical deposition in said index aperture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910198939A CN102062710B (en) | 2009-11-17 | 2009-11-17 | Preparation method of observation sample for transmission electron microscope |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910198939A CN102062710B (en) | 2009-11-17 | 2009-11-17 | Preparation method of observation sample for transmission electron microscope |
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| CN102062710A CN102062710A (en) | 2011-05-18 |
| CN102062710B true CN102062710B (en) | 2012-09-19 |
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| CN200910198939A Expired - Fee Related CN102062710B (en) | 2009-11-17 | 2009-11-17 | Preparation method of observation sample for transmission electron microscope |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103021802B (en) * | 2011-09-23 | 2015-06-17 | 中芯国际集成电路制造(上海)有限公司 | Production method for detection sample of semiconductor device, and detection sample |
| CN102680742A (en) * | 2012-05-28 | 2012-09-19 | 上海华力微电子有限公司 | Method for labeling atomic force nano-probe sample and method for manufacturing integrated circuit |
| CN103776669B (en) * | 2012-10-26 | 2016-08-03 | 中芯国际集成电路制造(上海)有限公司 | The preparation method of TEM sample |
| CN104344980A (en) * | 2013-07-29 | 2015-02-11 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of electron microscope scanning sample |
| CN104792584B (en) * | 2014-01-17 | 2017-08-29 | 中芯国际集成电路制造(上海)有限公司 | A kind of preparation method of TEM sample |
| CN104451824B (en) * | 2014-11-28 | 2017-01-18 | 四川大学 | Method and application of peeling titanium surface coating by adopting nanotube treatment method |
| CN104777024B (en) * | 2015-04-23 | 2017-09-19 | 上海华力微电子有限公司 | The preparation method and localization method of a kind of transmission electron microscope sample |
| CN105352768A (en) * | 2015-09-27 | 2016-02-24 | 上海华力微电子有限公司 | TEM sample positioning method |
| CN106289909B (en) * | 2016-08-19 | 2019-01-22 | 上海华力微电子有限公司 | The method for preparing example of transmission electron microscope |
| CN107894357B (en) * | 2017-11-08 | 2021-03-05 | 上海华力微电子有限公司 | Automatic sample thinning method |
| CN112083022A (en) * | 2019-06-12 | 2020-12-15 | 苏试宜特(上海)检测技术有限公司 | Specific micro-area calibration method based on plane sample rotary section sample |
| CN111366428B (en) * | 2020-03-03 | 2023-06-09 | 上海华力集成电路制造有限公司 | Method for preparing TEM sample by FIB (fiber reinforced plastic) inverted cutting |
| CN112146953B (en) * | 2020-09-21 | 2024-03-01 | 长江存储科技有限责任公司 | Test sample and preparation method thereof |
| CN113820578B (en) * | 2021-09-14 | 2024-02-20 | 长江存储科技有限责任公司 | Method for measuring semiconductor device |
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